Method of making a size



Nov. .1, 1938. A. c. DREsHr-IELD E1- AL METHOD oF MAKING A SIZE Filed May 11, 1935 Patented Nov. 1, 1938 UNITED STATES METHOD oF MAKING A sTzE Arthur C. Dreshfield,

Kalamazoo, Mich., and

Henry A. Johnstone, Savannah, Ga., assignors, lby mesne assignments, to Hercules Powder Company, Wilmington, Del., a corporation of Delaware Application May 11,

8 Claims.

This application is aA continuation in part of our application, Serial No. 569,216, led October 16, 1931.

This invention relates to an improvement in a method of making a rosin size.

larly, this invention relates to rosin size characterized by various novel and advantageous characteristics and to a novel and highly eiiicient method and apparatus for producing rosin size.

Generally speaking, the paper size in accordance with our invention comprises a reaction product of abietic acid, or equivalently of rosin, and caustic alkali, the reagents being reacted in proportions such that the rosin size product is 1J free or substantially free of saponiable substance, i. e., more particularly, free or substantially free of unsaponified rosin and/or excess or unreacted caustic alkali.

The rosin size product in accordance with our invention is more specifically characterized by the fact that it is in the form of non-tacky, discrete particles having a cellular structure rendering them porous, and a minimum moisture content. The rosin size product is essentially dry and .35 at the same time, by virtue of its characteristics indicatedand more particularly by virtue of the cellular structure of the discreteparticles, is rapidly and completely soluble in cold water.

The rosin size in accordance with our invengg tion is of substantial advantage from the practical standpoint inasmuch as it will not deteriorate in shipment or storage and can be packed in paper bags, and inasmuch as it may be dissolved in Water rapidly and easily Without the y.; necessity for heating, mechanical agitation, or

other aids heretofore found necessary in dissolving rosin sizes.l

The process in accordance with our invention, generally speaking, involves the saponiiication of 11) abietic acid or rosin with caustic alkali and on completion of the saponication, discharging the reaction mass under maintained pressure and temperature into an atmosphere maintainedat a relative humidity below or about 78%, it hav- .;3 ing been found that a relative humidity of. be-

low or about '78% is critical for the production of a rosin size having the characteristic of substantial dryness or low moisture content possessed by the rosin size contemplated by our :11i invention. In other words, the rosin size in accord-ance with our invention can be produced where the reaction mass is discharged into an atmosphere having a relative humidity below or about 78%. By relative humidity, we mean F3 the weight oi water vapor, expressed as a percentage, contained in a given volume` of air, divided by thc weight which would be ,contained in the same volume .of saturatedair at the same temperature.

60 For preferred operation, therelative humidity More particu- A 1935, Serial No. 21,024

is maintained about or below 72% and this secures vvery satisfactory results. As the relative 4humidity rises above this, less desirable results are secured and'when the relative humidity exceeds 78% or 80%, the dry matter decreases rapidly, and therefore, We recommend and in practice aim to maintain the relative humidity at aboutv 7.2% or below. Superheat or superheating is used here to dene the step in the method or process of heating a mass containing water to a temperature above its atmospheric boiling point without converting the Water intoI vapor by' maintaining the vheated mass under pressure.

More particularly, the method in accordance With our invention comprises discharging the superheated saponified abietic acid or rosin under pressure and at a temperature such as above indicated into an enclosed chamber, through which air maintained at a relative humidity below or about 78%, which is critical; is circulated. Various more specific details comprised in the process in accordance with our invention will appear from the more detailed description thereof hereinafter.

The apparatus embodying our invention from the broad standpoint comprises a combination of elements wherein the saponiiication of abietic acid or rosin with caustic alkali is effected, for such heating as above indicated under pressure, for discharging ,the reaction mass, for receiving the discharged size and forinsuring the maintenance of the relative humidity of the atmosphere intowhich the reaction mass or size is discharged at or below about the critical relative humidity of '78%,

Further and more specic details of the apparatus in accordance with our invention will be m-adeapparentfrom the detailed description of a preferred embodiment'thereof hereinafter.'

Having thus indicated in a general way the nature and purpose of this invention, we will proceed to a more detailed description theeof with reference to the accompanying drawing, in which:

The single gure is a fragmentary view in side elevation of an apparatus embodying the invention and adapted for the carrying out of our process for the production of the product.

Referring to the drawing, I indicates an autoclave provided with a pressure gauge 2 and an agitator 2.2 driven as shown from a motor 24. The autoclave is jacketed, the jacket being connected with a supply of heating medium, preferably steam, through a conduit 4 and with an outlet conduit 5. The top of the autoclave is also connected with a supply or source of air under pressure through a conduit 6 and with a relief valve 1. The autoclave is adapted for reacting abietic acid or rosin with a solution of caustic alkali for the production of a rosin size.

Suitably supported above the autoclave is a tank 8 adapted to hold a supply of roin. The tank 8 is formed with a heating medium jacket or provided with steam coils (not shown) whereby rosin supplied to the tank 8 may be melted and maintained in a molten condition. The tank 8 is connected to the autoclave by means of a valved conduit 9, by which molten rosin in a predetermined batch or quantity may be run into the autoclave. Adjacent the autoclave is positioned a tank I0 adapted to contain a supply of caustic soda solution. The tank I0 is connected with a supply or source of air under pressure through a valved conduit II and the tank is also connected with the bottom of the autoclave by a valve conduit I2. It will be noted that caustic soda solution in tank I0 may be discharged into the autoclave by means of air pressure admitted to tank I0 through conduit II.

An enclosed blow chambers I3 has projecting into it a discharge nozzle I4. The nozzle is connected through a valved conduit I5 with the bottom of the autoclave. The bottom of the chamber I3 is preferably formed in a V-shape and is provided with a longitudinal opening at its low point through which the product I5 collecting in the chamber falls upon a conveyor belt I`I by which the product is carried to a convenient place for packing or storage.

The blow chamber I3 is provided with means for the admission of air, such, for example, as louvers I8, adjacent which are positioned heating elements I9 adapted to be connected to a suitable source of heat, as for example, steam.

Alternatively, the heating elements may be replaced by electrical heating elements or the like, by which the temperature of the air entering the chamber I3 may be raised.

From the top of the chamber, a conduit 20 leads to the suction side of a suitably driven exhaust blower 2I by which air is drawn through the chamber. The discharge from the -blower 2I is connected to a conduit 22 leading to a separator 23. .In the conduit 20, through which, as has been indicated, air is drawn from the chamber by the blower 2|, and preferably adjacent the point of connection of the conduit 20 with the chamber, is placed a humidostat 25, adapted to respond to the relative humidity of the air leaving the chamber I3. By any suitable arrangement, electrical or otherwise, the humidostat 25 is arranged to control the temperature of the air entering the chamber through the louvers I8 by control of the heating elements I9. An air dehydrating means might be employed, but the apparatus as illustrated is highly practical.

The heating of the incoming air into the blow chamber is not for the purpose of heating the air but merely for the purpose of maintaining the desired degree of relative humidity. In practice, it is preferred that the temperature of the air passing through the blow chamber shall not exceed F. for best results and in any event, it should be well below the temperature of the saponified resin discharged into the chamber. For the plant or apparatus described, the volume of ,air drawn through the blow chamber should at least be 1200 cubic feet per minute.

With respect to the apparatus above described, it will be appreciated that the apparatus may comprise a single autoclave and means of discharge, in which case the chamber I3 will be oi suitable size relative to the capacity of the autoclave, or a plurality of autoclaves and means of discharge may be associated with a single chamber of a size relative to the combined capacity of the autoclaves, or the several reaction means may be manipulated to effect a continuous discharge to the chamber.

'A typical installation, for example,` may comprise a series of ve autoclaves arranged in line adjacent one end of a drying chamber, each autoclave being provided with a discharge nozzle within the chamber. In such an installation, assuming that the combined capacity of the autoclavcs is five tons of finished product per charge, the chamber I3 should be about fty feet long, thirty feet wide and forty feet high, and desirably the walls of the chamber are insulated in order to avoid loss of heat therethrough. For an installation of this capacity the volume of air drawn through the blow chamber should be at least 12,000 cubic feet per minute.

In the operation of the apparatus in accordance with our invention, as detailed above, for the carrying out of the method in accordance with our invention, molten rosin from the tank B' is run into the autoclave I. The rosin is heated to a temperature of about 275 F. before its introduction into the autoclave, and the autoclave, through the introduction of heating medium through conduit 4 into its jacket, is brought to a similar temperature. The tank I0 contains an aqueous solution of caustic soda of a concentration within about the range of 25% to about 50% (preferably 40%) caustic soda, by weight, and the solution in tank I0 is brought to a temperature of about 220 F. to 275 F. by

any suitable means, such as a steam coil (not shown) within the tank.

Molten rosin in a desired quantity having been introduced into the autoclave, an amount of caustic soda solution containing an amount of caustic suiilcient to saponify the amount of rosin previously introduced into the autoclave is then blown into the bottom of the autoclave through conduit I2, by the introduction of air under pressure into the tank I0, through conduit II. The amount of caustic soda is such that on completion of saponication the product does not contain in excess of about 2.5% free rosin or 0.5% free caustic soda. We nd that 12.1% of dry alkali based on dry rosin is preferable for gum rosin and 11.7% for wood rosin, depending upon their saponication number.

The caustic soda solution is blown upwardly through the molten rosin in the autoclave and the agitator 3 in the autoclave is operated to intermingle the rosin and the solution while, at the same time, the temperature within the autoclave is maintained within the range o1' 275 F. to 375 F. until saponication is completed. During the reaction in the autoclave, a pressure which is due largely to the evolution of steam from the water of the caustic solution at the temperature used is maintained. This pressure is' preferably held between 100 pounds and 125 pounds gauge for the temperature stated.

It will be noted that the reaction is carried out in the autoclave under pressure and in the absence of air, i. e., in thc presence of the steam and vapor evolved from the reaction mass. When the reaction is complete, the reaction mass or saponified rosin within the autoclave contains about 15% to 20% moisture, it being noted that loss of any substantial amount of moisture is avoided. Hence, hardening and stiiening oi' the 75 reaction mass is avoided and the latter is in a mobile state due to its moisture content.

On completion of the reaction, the reaction mass is further agitated in the autoclave by means of the agitator to render it homogeneous, and then the mass is discharged into the chamber I3 through the nozzle I4, a il-attened pipe having been found to be-very satisfactory, the discharge being effected under constant pressure through conduit I5 by the introduction of air under pressure at the top of the autoclave through the conduit 6. The discharge pressure is preferably held between 100 pounds and 125 pounds gauge.

Prior to the discharge of the saponified rosin into the chamber I3, the blower 2| is started and a circulation of air through the chamber is set up. It will be noted that air enters the chamn ber through the louvers I8 and is withdrawn therefrom through conduit 20. As the circulationoi air st-arts, the humidostat 25 respondsto the relative humidity of the air. The humidostat, being arranged to control temperature of the air entering the chamber through the louvers I8 through control of the heating elements IB, is adjusted to maintain the relative humidity of the air passing out of the chamber and consequently the air within the chamber at or be low '78%.

The saponified rosin is discharged into the chamber I3 in a finely subdivided state. The finelysubdivided particles are of a substantially uniform size,.and since the interior of the chamber is under atmospheric pressure, there is a sudden reduction in pressure on, and the simultaneous fine subdivision of, the superheated saponied rosin, the moisture therein, due to the superheat of the mass, expands or flashes into steam and at the same time there is a similar instantaneous and rapid expanion of gases or vapors present in the mass. ,As a consequence, the finely subdivided particles are dried or` relieved of moisture and of volatile products in the form of gases or vapors. Further, as a result of the rapid expansion resulting in the release of moisture and gas or vapors, the finely subdivided particles are given a cellular structure and instantly cooled which prevents any deleterious action which might result from prolonged exposure to heat.

As the saponfied rosin is discharged into the chamber and the finely subdivided particles thereof are relieved of moisture and gases and vapors, the moisture and gases or vapors are carried out oi the chamber under the influence of the blower 2| through the conduit 20 and the dry inelyl divided particles of saponiiied rosin having a cellular structure fall to the bottom of the-chamber and pass to the conveyor belt I1.

The moisture removed from th'e finely subdivided particles o f saponified rosin, which is picked up and carried from the chamber I3 by the air circulating therethrough, tends to increase the relative humidity of the air inthe chamber. In-

creasing the relative humidity of the air in the chamber to a point above about '78% relative humidity causes the humidostat in conduit 20 to exert a control upon the heating elements I9, such that thev temperature of the air in the chamber is increased and consequently also the 'relative humidity of the air in the chamber maintained at or below about r(8%.

It will be noted that in practical operation the -relative humidity of the air in the chamber I3 is fixed well below the 78% before discharge of saponlfled rosin thereinto and that the heating elements I9 controlled by the humidostat are arranged so that the relative humidity in the chamber is not at any time permitted to exceed about 78% relative humidity during the discharge of saponifed rosin into the chamber.

The air leaving the chamber I3 through the conduit 20 carries some ne particles of the dried rosin size, such particles, however, being recovered in the separator 23 through which the air is discharged.

It will be appreciated that Various modifica tions may be made in the apparatus as detailed above and in the carrying out of the process as detailed above, without departure from the scope of,

our invention.

The procedure in accordance with our invention is of especial advantage in enabling the production of a high grade size with wood rosin, as, for example, FF rosin, or even low grade B wood rosin, since the greenish coloring matter of the wood rosin, heretofore carried into the size and paper treated therewith, is volatilized, destroyed,V

or removed from the size under the conditions of production in accordance with our invention.

It will be appreciated that from the process standpoint our invention comprises essentially discharging and drying superheated saponified abietic acid or rosin in an atmosphere having a relative humidity not in excess of 78%, and that from the apparatus standpoint our invention comprises essentially a combination of elements for the saponification and discharge of abietic acid or rosin and for controlling the relative humidity of the atmosphere in which the saponified abietic acid or rosin is discharged within the limit contemplated by the process.

The rosin size made in accordance with our,

invention comprises, as has been indicated, discrete particles having a cellular structure rendering them porous. The particles are characterized by the fact that they are non-tacky, by the fact that they are substantially dry or have a moisture content not in excess of about 8%, by their substantial freedom from saponiiiable substances, more particularly, no more than 2.5% of unsaponied rosin or 0.5% of caustic alkali, and by their rapid solubility in cold water and is substantially free from volatile organic matter. The product is also characterized by the fact that it comprises abietic acid or rosin saponied with a caustic al kali solution.

By virtue of the fact that the various condi,- tions effecting the result are under control before, during and after discharge, we are able to lobtain uniformly a product having the desired properties. We refer to the control of the material in the autoclave and in the drier.

As stated, they size produced by this method is characterized by being free or substantially free' of saponiiiable substances, is in the form of non- .tacky discrete particles having a cellular structure 1. The method of producing a readily watersoluble dry rosin size which is characterized by being in the form of discrete porous particles which comprises saponifying rosin with a substantially chemically equivalent amount of an aqueous solution of caustic alkali, heating the saponifying materials to a temperature between about 275 F. and about 375 F. and ,under a pressure between about pounds gauge and about 125 pounds gauge, whereby a saponified rosin having a water content between about 15% and 20% is produced, discharging said saponied rosin while under said pressure and said temperature into a zone, maintained under substantially atmospheric pressure, and in which the atmosphere is maintained with a relative humidity not in excess of about 78%, whereby the saponified rosin is deprived of most of its moisture content and the said dry size produced.

2. The method of producing a readily watersoluble dry rosin size which is characterized by being in the form of discrete porous particles which comprises saponifying abietic acid with a substantially chemically equivalent 'amount of lan aqueous solution of caustic alkali, heating the saponifying materials to a temperature between about 275 F. and about 375 F. and under a pressure between about 100 pounds gauge and about pounds gauge whereby a saponied abietic acid having a water content between about 15% and 20% is produced, discharging said saponied abietic acid while under said pressure and said temperature into a zone, maintained under substantially atmospheric pressure, and in which the atmosphere is maintained with a relative humidity not in excess of about 78%, whereby the saponiiled abietic acid is deprived of most of its moisture content and the said dry size produced.

3. 'I'he method of producing a readily watersoluble dry rosin size which is characterized by being in the form of discrete porous particles which comprises saponifying rosin with a substantially chemically equivalent amount of an aqueous solution of caustic alkali, heating the saponifying materials to a temperature between about 275 F. and about 375 F. and under a pressure between about 100 pounds gauge and about 125 pounds gauge, whereby a saponified rosir` having a water content between about 15% and 20% is produced, discharging said saponied rosin while under said pressure and said temperature in to an atmosphere maintained under substantially atmospheric pressure, at a temperature below that o1' the saponified rosin, and with a relative humidity not in excess of about 78%, whereby the saponied rosin is deprived of most of its moisture content and the said dry size produced.

4. The method of producing a readily watersoluble dry rosin size which is characterized by being in the form of discrete porous particles which comprises saponifying abietic acid with a substantially chemically equivalent amount of an aqueous solution of caustic alkali, heating the saponifying materials to a temperature between about 275 F. and about 375 F. and under a pressure between about 100 pounds gauge and about 125 pounds gauge, whereby a saponified abietic acid having a water content between about 15% and 20% is produced, discharging said saponied abietic acid while under said pressure and said temperature into an atmosphere maintained under substantially atmospheric pressure, at a temperature below that of the saponied abietic acid,

and with a relative humidity not in excess of about 78%, whereby the saponied abietic acid is deprived of most of its moisture content and the said dry size produced.

5. The method of producing a dry rosin size in the form of discrete porous particles, which comprisessaponifying rosin with an aqueous 4solution of caustic alkali, superheating the saponifying mixture under a temperature between about 275 F. and about 375 F. and under a pressure of about 100 pounds to about 125 pounds gauge, discharging the superheated saponified rosin having a water content of about 15% to about 20% while under said pressure and at said temperature into a cooling atmosphere maintained at a relative humidity not in excess of about 78% and -under a substantially lower pressure whereby the saponied rosin is deprived of most of its moisture content and the said dry size produced.

6. The method of producing a dry rosin size, which comprises saponifying rosin with an aqueous solution of caustic alkali, and discharging the saponied rosin having a water content of about 15% to about 20% while at a temperature between about 275 F. and about 375 F. and at a pressure of about 100 pounds to about 125 pounds gauge into an enclosed chamber while circulating in said chamber air which is under a substantially lower pressure than that of the saponied rosin and which has been heated to a temperature below that of the discharged saponified rosin and which has a 'relative humidity below about 78%, whereby the saponified rosin is deprived of most of its moisture content and the said dry size produced.

7. The method of producing a dry rosin size,

which comprises saponifying wood rosin with an aqueous solution of caustic alkali, and discharging the saponied rosin having a water content of about 15% to about 20% while at a temperature between about 275 F. and about 375 F. and under a pressure of about 100 pounds to about 125 pounds gauge into anenclosed chamber while circulating therein air which is under a substantially lower pressure than that of the saponifled rosin and which has been heated, but to a temperature below ythat of the discharged saponied rosin and which has a relative humidity below about 78%, whereby moisture, coloring matter and volatile bodies are removed from the size and the size is produced in the form of discrete, porous and substantially dry particles.

8. A process` for producing a dry porous and readily soluble rosin size which comprises the steps of introducing rosin and saponifying materials under pressure into a closed reaction chamber, applying heat and pressure to produce within said reaction chamber a temperature within the range of about 275 F. to about 375 F. and a pressure within the range of about 100 pounds gauge to about 125 pounds gauge, and discharging the saponied material from the said reaction chamber by said pressure maintained therein into a iiash chamber, in which a cooling atmosphere is maintained at a lower temperature and pressure and at a relative humidity not in excess of about 78%, the moisture content of the saponied materia] being so diminished thata dry size results, said dry size being characterized by moisture content not in excess of 8% and by being in the form of discrete porous particles.

ARTHUR C. DRESHFIELD.

HENRY A. JOHNSTONE. 

